HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 12074212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 378892 | HCID 378892 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 12074212 | HCID 12074212 | 92% |
Reaction Steps
A solution of 4-fluoro-2-nitro-1-(phenylsulfonyl) benzene (1.0 g, 3.6 mmol), piperazine (0.37 g, 4.3 mmol), and potassium carbonate (0.79 g, 5.7 mmol) is stirred in 35 mL of acetonitrile overnight at reflux. The mixture is cooled to rt and 35 mL of water and CH2Cl2 are added. The layers are separated and the aqueous layer extracted with CH2Cl2 (3×35 mL). The combined organics are dried over MgSO4, filtered, and concentrated. Purification via flash column chromatography (15% MeOH/CH2Cl2) gives 1.1 g (92%) of title compound as a solid, mp 180-182° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06579870B2 |
| Source dataset | uspto-grants-2003_06 |
| ORD ID | ord-975cd5d7bb8b4c5f89fcd9202c08cfed |
| Source note | uspto-grants-2003_06 |